Reaktion #1736742

Reaktionsgleichung

triethylamine

N-methyl-N-trichloromethylthio-carbamoyl fluoride

1-methyl-4-hydroxypyrazole

→

N-methyl-N-trichloromethylthiocarbamic acid O-(1-methyl-pyrazol-4-yl) ester

Ausbeute 86.6%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted twice with 25 ml of water each time
2. 2
   TrocknenThe organic phase was dried over sodium sulphate
3. 3
   Sonstigeevaporated in vacuo
4. 4
   workup.DISTILLATIONThe residue was subjected to incipient distillation under a high vacuum

Vorschrift

5.1 g (0.05 mol) of triethylamine were added dropwise to a mixture of 11.3 g (0.05 mol) of N-methyl-N-trichloromethylthio-carbamoyl fluoride, 4.9 g (0.05 mol) of 1-methyl-4-hydroxypyrazole and 150 ml of toluene. After 4 hours, the mixture was extracted twice with 25 ml of water each time. The organic phase was dried over sodium sulphate and evaporated in vacuo. The residue was subjected to incipient distillation under a high vacuum. 12.5 g (82% of theory) of N-methyl-N-trichloromethylthiocarbamic acid O-(1-methyl-pyrazol-4-yl) ester were thus obtained in the form of a yellow oil with a refractive index nD23 of 1.5492.

Quelle